Commission Regulation (EC) No 2074/2005 of 5 December 2005 laying down implementing measures for certain products under Regulation (EC) No 853/2004 of the European Parliament and of the Council and for the organisation of official controls under Regulation (EC) No 854/2004 of the European Parliament and of the Council and Regulation (EC) No 882/2004 of the European Parliament and of the Council, derogating from Regulation (EC) No 852/2004 of the European Parliament and of the Council and amending Regulations (EC) No 853/2004 and (EC) No 854/2004 (Text with EEA relevance)
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Reference procedure
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Version Superseded: 14/12/2019
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Point in time view as at 01/07/2011.
Changes to legislation:
There are currently no known outstanding effects for the Commission Regulation (EC) No 2074/2005,
Reference procedure
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Reference procedure U.K.
1.Purpose and area of applicationU.K.
This method describes a reference procedure for identifying the nitrogen concentration of TVB-N in fish and fishery products. This procedure is applicable at TVB-N concentrations of 5 mg/100 g to at least 100 mg/100 g.
2.DefinitionU.K.
‘TVB-N concentration’ means the nitrogen content of volatile nitrogenous bases as determined by the procedure described.
The concentration shall be expressed in mg/100 g.
3.Brief descriptionU.K.
The volatile nitrogenous bases are extracted from a sample using a solution of 0,6 mol perchloric acid. After alkalinisation the extract undergoes steam distillation and the volatile base components are absorbed by an acid receiver. The TVB-N concentration is determined by titration of the absorbed bases.
4.ChemicalsU.K.
Unless otherwise indicated, reagent-grade chemicals should be used. The water used must be either distilled or demineralised and of at least the same purity. Unless otherwise indicated, ‘solution’ means an aqueous solution as follows:
(a)
perchloric acid solution = 6 g/100 ml;
(b)
sodium hydroxide solution = 20 g/100 ml;
(c)
hydrochloric acid standard solution 0,05 mol/l ((0,05 N),
Note:
When using an automatic distillation apparatus, titration should take place with a hydrochloric acid standard solution of 0,01 mol/l ((0,01 N);
(d)
boric acid solution = 3 g/100 ml;
(e)
silicone anti-foaming agent;
(f)
phenolphtalein solution = 1 g/100 ml 95 % ethanol;
(g)
indicator solution (Tashiro Mixed Indicator) 2 g methyl-red and 1 g methylene-blue are dissolved in 1 000 ml 95 % ethanol.
5.Instruments and accessoriesU.K.
(a)
A meat grinder to produce a sufficiently homogenous fish mince.
(b)
High-speed blender with a speed of between 8 000 and 45 000 revolutions/min.
(c)
Fluted filter, diameter 150 mm, quick-filtering.
(d)
Burette, 5 ml, graduated to 0,01 ml.
(e)
Apparatus for steam distillation. The apparatus must be able to regulate various amounts of steam and produce a constant amount of steam over a given period of time. It must ensure that during the addition of alkalising substances the resulting free bases cannot escape.
6.ExecutionU.K.
Warning: When working with perchloric acid, which is strongly corrosive, necessary caution and preventive measures should be taken. The samples should, if at all possible, be prepared as soon as possible after their arrival, in accordance with the following instructions:
(a)
Preparing the sample
The sample to be analysed should be ground carefully using a meat grinder as described in point 5(a). Exactly 10 g +0,1 g of the ground sample is weighed out into a suitable container. This is mixed with 90,0 ml perchloric acid solution as specified in point 4(a), homogenised for two minutes with a blender as described in point 5(b), and then filtered.
The extract thereby obtained can be kept for at least seven days at a temperature of between approximately 2 oC and 6 oC;
(b)
Steam distillation
50,0 ml of the extract obtained in accordance with point (a) is put into an apparatus for steam distillation as described in point 5(e). For a later check on the extract's alkalinisation, several drops of phenolphtalein as specified in point 4(f) are added. After adding a few drops of silicone anti-foaming agent, 6,5 ml of sodium hydroxide solution as specified in point 4(b) is added to the extract and steam distillation begins immediately.
The steam distillation is regulated so that around 100 ml of distillate is produced in 10 minutes. The distillation outflow tube is submerged in a receiver with 100 ml boric acid solution as specified in point 4(d), to which three to five drops of the indicator solution as described in point 4(g) have been added. After exactly 10 minutes, distillation is ended. The distillation outflow tube is removed from the receiver and washed out with water. The volatile bases contained in the receiver solution are determined by titration with standard hydrochloric solution as specified in point 4(c).
The pH of the end point should be 5,0+0,1.
(c)
Titration
Duplicate analyses are required. The applied method is correct if the difference between the duplicates is not greater than 2 mg/100 g.
(d)
Blank
A blind test is carried out as described in point (b). Instead of the extract, 50,0 ml perchloric acid solution as specified in point 4(a) is used.
7.Calculation of TVB-NU.K.
By titration of the receiver solution with hydrochloric acid as in point 4(c), the TVB-N concentration is calculated using the following equation:
V1 = Volume of 0,01 mol hydrochloric acid solution in ml for sample
V0 = Volume of 0,01 mol hydrochloric acid solution in ml for blank
M = Weight of sample in g.
Remarks
1.Duplicate analyses are required. The applied method is correct if the difference between duplicates is not greater than 2 mg/100 g.U.K.
2.Check the equipment by distilling solutions of NH4Cl equivalent to 50 mg TVB-N/100 g.U.K.
3.Standard deviation of reproducibility Sr = 1,2 mg/100 g. Standard deviation of comparability SR = 2,50mg/100 g.U.K.
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